Preparation Of Organotextile Catalyst And Its Application For Williamson Ether Reaction In Phase Transfer Catalysis System

Phase Transfer Catalysis(PTC)is one of the most important catalytic technologies in the industrial field.It has the advantages of fast reaction rate,high yield and convenient product handling.By adding a catalytic amount of a third substance namely phase transfer catalyst,the reactant can be transferred from one phase to the other and reacted with the other reactant in the latter phase,resulting in the homogeneous reaction.PTC technology has the disadvantages of difficult reuse of catalyst,low reaction efficiency and high energy consumption.With the increasing urgency of energy saving,emission reduction and high efficiency requirements in the chemical industry,the improvement of the efficiency and reusability has also become a hot and difficult issue in the field of PTC.The catalyst immobilization and the serialization are the most commonly-used way for energy savingemission reduction,high efficiency in Conventional heterogeneous catalytic reaction system.In this paper,combined with the process of pad printing in dyeing and finishing,a new method of continuous catalysis with fiber as catalyst loading carrier is proposed.First of all,cotton fiber and modified acrylic fiber are used as the carrier,and the organic catalytic fiber is prepared by cationic modification of the fiber surface.The preparation process of the cationic modifier and the organic catalytic fiber are discussed.The morphology and adsorption properties of the organic catalytic fiber,the catalytic performance of organic catalytic fibers in the synthe-sis of Williamson ether was studied.Finally,the catalytic performance of the organic catalytic fibers in different reaction substrates and the recycle performance of the catalyst were compared to provide a continuous and efficient PTC reaction system new ideas,the primary result are as follows.(1)Trimethylamine,triethylamine,tripropylamine,N,N-dimethylbutylamine,N,N-dimethyl-benzylamine,N,N-dimethyl-n-octylamine and N,Dialkyl amine as raw materials,reacted with epichlorohydrin to prepare seven kinds of 3-chloro-2-hydroxypropyl trialkylammonium chloride(CHTPAC)cationic modifier.The effects of different reaction conditions such as temperature,time,the effect of dosage ratio on the yield of the reaction was investigated.The structure of the product was characterized by using nuclear magnetic resonance spectroscopy(NMR),and the reaction process was analyzed.The results showed that the reaction of trialkylamine with epichlorohydrin increased with the increase of the length of trialkylamine,the steric hindrance of trialkylamine increased and the reaction difficulty increased.For the short-chain alkyl CHPTAC reaction,the ratio of raw materials was 1:1,the reaction temperature is 35?,the reaction for 2 h,the yield of more than 95%.While the long chain alkyl CHPTAC ratio of 1:4,the reaction 15 h,the yield can reach more than 80%.Larger trialkylamine due to changes in the pH value of the reaction system,the presence of CHPTAC and epoxy compounds in the product,through the conversion of concentrated hydrochloric acid can be achieved between them.(2)Organic catalysis fibers were prepared by using CHPTAC as modifier,cotton fiber and aramid fiber as matrix.The effects of different modification methods(impregnation method,padding method),process conditions(CHPTAC dosage,NaOH dosage,temperature).The morphology and structure of the catalytic fiber were characterized by SEM,FTIR and Zeta potential.The results showed that the padding method was more suitable for the preparation of organic catalytic fibers.The optimum conditions were as follows:the dosage of CHPTC was 100 g/L,the mass ratio of quaternary ammonium cation etherifying agent to NaOH was 1:2,the rate of liquid was 70%curing process 4 h in 80?.The modified fiber possesses the adsorption capacity of up to 600 mg/g for acid dye and the catalytic fiber prepared from acrylic fiber with 5%Compared with fibrils.The organic catalytic fibers showed an increase in surface roughness and little change in the overall structure.The surface of modified organic fibers possessed a certain positive charge.However,the charge of organic catalytic fibers prepared from modified acrylic fibers was significantly larger than the of cotton fibers.(3)Based on the Williamson ether synthesis of phenol derivatives and benzyl chloride derivatives,the catalytic properties of two types of organic catalytic fibers were investigated.The effects of different reaction conditions(temperature,solvent and catalytic fiber)on the catalytic activity influence,compared with the phenolic substrate expansion,catalytic fiber changes in the catalytic performance.The results showed that two types of catalysis fibers showed high adsorption capacity for phenol with adsorption capacities of 50 mg/g and 30 mg/g,respectively.Two kinds of catalytic fibers catalyzed the synthesis of Williamson ether with dichloromethane or toluene as solvent,when the molar ratio of phenol to benzyl chloride was 1:1.1,the yield was 96%after 3 h of reflux reaction.Two organic catalysis fibers catalyzed the synthesis of p-cresol,p-chlorophenol,o-chlorophenol and benzyl chloride.The reaction showed a high catalytic activity,the reaction yield was greater than 90%;two kinds of catalytic fiber reuse 10 times,the yield is still higher than 80%,and there is no significant changes in fiber strength.